EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0049

Report generated Sep 08, 2006; 07:39:58

Unit cell

2447 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)5.3807 +/- 0.0003
b (Angstrom)8.1543 +/- 0.0006
c (Angstrom)12.6571 +/- 0.0011
alpha (°)78.351 +/- 0.004
beta (°)82.960 +/- 0.004
gamma (°)84.492 +/- 0.004
Volume (A**3)538.35 +/- 0.07
Mosaicity (°)0.691 +/- 0.004

Data collection

Summary

Total number of images collected364
Total exposure time11.0 hours
Data collection exposure time10.9 hours
Data collection wall-clock time11.4 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f139278.0° phi2.000°110 secondsYes
data collections02f33 66.0° omega2.000°110 secondsYes
data collections03f23 46.0° omega2.000°110 secondsYes
data collections04f53106.0° omega2.000°110 secondsYes
data collections05f54108.0° omega2.000°110 secondsYes
data collections06f54108.0° omega2.000°110 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected 312
Zero sigma or profile test  35
Overload or incomplete profile 626
Sigma cutoff  29
High resolution limit  21

Final Data Set

Scale factor range7.27-25.00
Number of 'full' reflections  7145
Number of 'partial' reflections  6534
Total number of integrated reflections 13057
Total number of unique reflections  2502
Data completeness  98.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   15.2
Average Sigma(I)    1.3
Overall R-merge (linear)  0.171

Sadabs Results

Parameter refinement on 5867 reflections reduced R(int) from 0.2184 to 0.1119

Before rejection, 12930 reflections total and 2516 unique

After rejection, 12525 reflections total and 2514 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.1624   0.565 - 1.126   0.928 - 1.475   1.368    4910    2298
    2   -7.8  0.0981   0.591 - 0.674   0.937 - 1.128   1.182    1132     684
    3   -7.8  0.0920   0.172 - 0.198   0.939 - 1.352   1.133     759     537
    4   -7.8  0.1573   0.627 - 1.221   0.933 - 1.303   1.386    1876     946
    5   -7.8  0.1916   0.584 - 0.930   0.938 - 1.303   1.448    1935     882
    6   -7.8  0.1983   0.885 - 1.462   0.941 - 1.298   1.411    1913     894
Ratio of minimum to maximum apparent transmission: 0.629048

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp7 c4  
  Formula   C9H14O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.14 x 0.06 x 0.02 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      SampleCode.hkl - data corrected using  SADABS
      SampleCode_merge_none.hkl - equivalents and friedels kept separate  (See "Final Data Set" table in this report)
      SampleCode.p4p - skeleton p4p file for use with XPREP
      SampleCode.htm - this summary file

Southampton CIF entry fields

_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 

Software References

Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an Obstinate List of Reflections. Journal of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from area-detector images. Journal of Applied Crystallography 2000; 33: 893-898.

Diffractometer control and strategy calculation using COLLECT:
Hooft RWW. COLLECT data collection software, Nonius B.V., 1998.

Standard Data Reduction using HKL(Denzo & Scalepack):
Otwinowski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt A. 1997; 276: 307-326.

Absorption Correction
Sheldrick, G. M. (2003). SADABS. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA.

Non-Standard Data Reduction using EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity evaluation method: EVAL-14. Journal of Applied Crystallography 2003; 36: 220-229.

For more information visit the service web site at: http://www.soton.ac.uk/~xservice/